CN115770878A - A method for reducing the anisotropy of the mechanical properties of additively manufactured high-strength titanium alloys - Google Patents
A method for reducing the anisotropy of the mechanical properties of additively manufactured high-strength titanium alloys Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于合金材料制备技术领域,具体涉及一种降低增材制造高强钛合金力学性能各向异性的方法。The invention belongs to the technical field of alloy material preparation, and in particular relates to a method for reducing the anisotropy of the mechanical properties of a high-strength titanium alloy manufactured by additive manufacturing.
背景技术Background technique
钛合金具有比强度高、生物相容性好、耐腐蚀、无磁性、耐热等优点,在生物医疗、航空航天、海洋工程、石油化工等领域获得了广泛应用。随着航空航天事业的快速发展,常规的钛合金材料难以满足其需求,于是高强钛合金进入了人们的视线。Titanium alloy has the advantages of high specific strength, good biocompatibility, corrosion resistance, non-magnetism, heat resistance, etc., and has been widely used in biomedical, aerospace, marine engineering, petrochemical and other fields. With the rapid development of the aerospace industry, conventional titanium alloy materials are difficult to meet its needs, so high-strength titanium alloys have entered people's sight.
钛合金的导热性差、变形抗力大、锻造温度范围窄、对氧的亲和力大等,使钛合金样件的制备存在诸多困难。粉末床电子束增材制造,也称为电子束选区熔化(SEBM),是20世纪90年代发展的先进制造技术,具有扫描速度快、高真空环境无污染、低残余应力等优点,特别适合钛合金等活性金属材料的直接成形。Titanium alloys have many difficulties in the preparation of titanium alloy samples due to their poor thermal conductivity, high deformation resistance, narrow forging temperature range, and high affinity for oxygen. Powder bed electron beam additive manufacturing, also known as electron beam selective melting (SEBM), is an advanced manufacturing technology developed in the 1990s. It has the advantages of fast scanning speed, no pollution in high vacuum environment, and low residual stress. It is especially suitable for titanium Direct forming of active metal materials such as alloys.
Ti-1Al-8V-5Fe(Ti185)合金属于亚稳β钛合金,具有较高的抗拉强度和剪切强度,广泛应用于航空紧固件和一些对于强度要求较高的零部件。此外,该合金相比于其他亚稳β钛合金,成本较低。但采用粉末床电子束增材制造成形Ti185合金,合金内部沿成形方向为粗大柱状晶组织,导致合金力学性能各向异性明显,这个问题严重制约了粉末床电子束增材制造及其制备钛合金的大规模发展和推广应用。Ti-1Al-8V-5Fe (Ti185) alloy is a metastable β-titanium alloy with high tensile strength and shear strength. It is widely used in aerospace fasteners and some components that require high strength. In addition, the alloy is less costly than other metastable β-titanium alloys. However, powder bed electron beam additive manufacturing is used to form Ti185 alloy. The interior of the alloy is a coarse columnar grain structure along the forming direction, resulting in obvious anisotropy of the mechanical properties of the alloy. This problem seriously restricts powder bed electron beam additive manufacturing and its preparation of titanium alloys. Large-scale development and promotion of applications.
发明内容Contents of the invention
本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种降低增材制造高强钛合金力学性能各向异性的方法。该方法通过向Ti185合金粉末添加铁粉末进行粉末床电子束增材制造制备钛合金,提高了合金的生长限制因子和凝固温度区间值,有利于钛合金中等轴晶的形成,同时降低β/α转变温度,促进钛合金纳米α强化相析出,从而提高了钛合金的强度,并降低了钛合金力学性能各向异性。The technical problem to be solved by the present invention is to provide a method for reducing the anisotropy of the mechanical properties of high-strength titanium alloys manufactured by additive manufacturing in view of the above-mentioned deficiencies in the prior art. The method prepares titanium alloy by adding iron powder to Ti185 alloy powder for powder bed electron beam additive manufacturing, which improves the growth limiting factor and solidification temperature interval value of the alloy, is beneficial to the formation of equiaxed crystals in titanium alloy, and reduces β/α at the same time The transition temperature promotes the precipitation of nano-α strengthening phase of titanium alloy, thereby improving the strength of titanium alloy and reducing the anisotropy of mechanical properties of titanium alloy.
为解决上述技术问题,本发明采用的技术方案为:一种降低增材制造高强钛合金力学性能各向异性的方法,其特征在于,通过增大Ti-1Al-8V-5Fe合金即Ti185合金粉末中的铁含量,采用粉末床电子束增材制造制备得到力学性能向同性的高强钛合金,该方法包括以下步骤:In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a method for reducing the anisotropy of the mechanical properties of high-strength titanium alloys manufactured by additive manufacturing, which is characterized in that, by increasing the Ti-1Al-8V-5Fe alloy, that is, the Ti185 alloy powder The iron content in the powder bed electron beam additive manufacturing is used to prepare a high-strength titanium alloy with isotropic mechanical properties. The method includes the following steps:
步骤一、向等离子旋转电极气雾化制备的球形Ti185合金粉末中加入铁粉末,然后采用行星式球磨机进行球磨得到混合粉末;Step 1. Add iron powder to the spherical Ti185 alloy powder prepared by plasma rotating electrode gas atomization, and then use a planetary ball mill to perform ball milling to obtain a mixed powder;
步骤二、绘制目标产物钛合金的三维模型,然后进行分层处理,沿着三维模型的高度方向切分成等厚的片层,并获得切层数据,再对各片层的内部扫描方式和扫描路径进行设计,获得切层扫描数据;Step 2. Draw the 3D model of the target product titanium alloy, and then perform layering processing, cut into slices of equal thickness along the height direction of the 3D model, and obtain the slice data, and then scan the internal scanning method and scan of each slice Design the path and obtain slice scanning data;
步骤三、将步骤二获得的切层数据和切层扫描数据导入粉末床电子束增材制造成形设备中,将步骤一中得到的混合粉末装入粉末床电子束增材制造设备的粉箱中,然后调平成形底板并对成形底板进行预热,成形底板的预热温度为700℃~720℃;Step 3. Import the slice data and slice scan data obtained in step 2 into the powder bed electron beam additive manufacturing forming equipment, and put the mixed powder obtained in step 1 into the powder box of the powder bed electron beam additive manufacturing equipment , and then level the forming base plate and preheat the forming base plate, the preheating temperature of the forming base plate is 700 ° C ~ 720 ° C;
步骤四、将步骤三中装入粉箱中的混合粉末铺设在预热后的成形底板上形成铺粉层,然后对铺粉层进行预热,铺粉层的预热温度为700℃~720℃;所述铺粉层的厚度与步骤三中切分的片层的厚度相同;Step 4. Lay the mixed powder loaded into the powder box in step 3 on the preheated forming bottom plate to form a powder layer, and then preheat the powder layer. The preheating temperature of the powder layer is 700°C to 720°C. ℃; the thickness of the powder layer is the same as the thickness of the cut sheet in step 3;
步骤五、根据步骤三中导入粉末床电子束增材制造成形设备中的切层数据和切层扫描数据,采用电子束对步骤四中经预热后的铺粉层进行熔化扫描,形成单层实体片层,然后将成形底板下降,且成形底板的下降高度与步骤四中切分的片层的厚度相同;Step 5. According to the slice data and slice scan data imported into the powder bed electron beam additive manufacturing forming equipment in step 3, the electron beam is used to melt and scan the preheated powder layer in step 4 to form a single layer Solid sheet, then the forming bottom plate is lowered, and the lowering height of the forming bottom plate is the same as the thickness of the sheet layer cut in step 4;
步骤六、重复步骤四中的铺粉工艺、预热工艺和步骤五中的熔化扫描工艺、成形底板下降工艺,直至各单层实体片层逐层堆积,形成粉末床电子束增材制造成形件,然后待成形底板的温度小于100℃时取出,利用高压气体去除粉末床电子束增材制造成形件表面的残留粉末,得到高强钛合金;所述高强钛合金水平方向的抗拉强度高于1317MPa,竖直方向的抗拉强度高于1303MPa,水平方向的抗拉屈服强度高于1241MPa,竖直方向的抗拉屈服强度高于1222MPa,断后伸长率高于5%,强度各向异性值不高于1.5。Step 6. Repeat the powder spreading process and preheating process in step 4 and the melting scanning process and forming base plate lowering process in step 5 until each single-layer solid sheet is piled up layer by layer to form a powder bed electron beam additive manufacturing shaped part , and then take it out when the temperature of the forming bottom plate is less than 100°C, use high-pressure gas to remove the residual powder on the surface of the formed part by powder bed electron beam additive manufacturing, and obtain a high-strength titanium alloy; the tensile strength of the high-strength titanium alloy in the horizontal direction is higher than 1317MPa , the tensile strength in the vertical direction is higher than 1303MPa, the tensile yield strength in the horizontal direction is higher than 1241MPa, the tensile yield strength in the vertical direction is higher than 1222MPa, the elongation after fracture is higher than 5%, and the strength anisotropy value is not higher than 1.5.
本发明采用等离子旋转电极气雾化制备的球形Ti185合金粉末为原料并加入铁粉末进行球磨混合得到混合粉末,然后经粉末床电子束增材制造制备得到力学性能向同性的高强钛合金。首先,本发明采用的等离子旋转电极气雾化制备的球形Ti185合金粉末球形度高,且粒径适合粉末床电子束增材制造设备,增材制造过程中该球形粉末易均匀铺展,进而有利于提高Ti185合金的组织均匀性;其次,本发明通过向球形Ti185合金粉末中加入铁粉,增大了合金的生长限制因子和凝固温度区间,有利于等轴晶的形成,同时,铁是β稳定元素,铁含量的增大降低了合金的β/α转变温度,结合粉末床电子束增材制造进行制备,有利于钛合金获得更细小的强化相α,降低了钛合金力学性能各向异性;而将球形Ti185合金粉末与铁粉末采用行星式球磨机进行球磨混合,有利于铁粉末均匀分布在Ti185合金粉末的表面,有利于提高产物钛合金的成分均匀性;再次,本发明的粉末床电子束增材制造过程中,通过对成形底板和铺粉层进行预热,并控制预热温度为700℃~720℃,使得制备的各单层实体片层均经过反复的热处理过程,有利于产物钛合金内部热应力逐步释放,进而钛合金内部组织趋于均一,同时对铺粉层的球形Ti185合金粉末先预热再熔化扫描,使得粉末之间产生粘连,避免电子束冲击造成铺粉层移动,提高了钛合金的层间结合力,并避免钛合金发生成分偏析,特别是Fe元素的偏析产生β斑缺陷,影响钛合金的强度。The invention uses the spherical Ti185 alloy powder prepared by gas atomization of a plasma rotating electrode as a raw material, adds iron powder for ball milling and mixing to obtain a mixed powder, and then prepares a high-strength titanium alloy with isotropic mechanical properties through powder bed electron beam additive manufacturing. First of all, the spherical Ti185 alloy powder prepared by plasma rotating electrode gas atomization adopted in the present invention has high sphericity, and the particle size is suitable for powder bed electron beam additive manufacturing equipment. Improve the uniformity of the structure of the Ti185 alloy; secondly, the present invention increases the growth limiting factor and the solidification temperature range of the alloy by adding iron powder to the spherical Ti185 alloy powder, which is beneficial to the formation of equiaxed crystals. At the same time, iron is β-stable Elements, the increase of iron content reduces the β/α transition temperature of the alloy, and the preparation combined with powder bed electron beam additive manufacturing is conducive to obtaining a finer strengthening phase α for the titanium alloy, which reduces the anisotropy of the mechanical properties of the titanium alloy; And spherical Ti185 alloy powder and iron powder adopt planetary ball mill to carry out ball milling and mixing, help iron powder to be evenly distributed on the surface of Ti185 alloy powder, help to improve the component uniformity of product titanium alloy; Again, powder bed electron beam of the present invention In the process of additive manufacturing, by preheating the forming base plate and powder layer, and controlling the preheating temperature at 700°C to 720°C, each single-layer solid sheet is subjected to repeated heat treatment, which is beneficial to the production of titanium. The internal thermal stress of the alloy is gradually released, and then the internal structure of the titanium alloy tends to be uniform. At the same time, the spherical Ti185 alloy powder in the powder layer is preheated and then melted and scanned to make the powders stick together and avoid the movement of the powder layer caused by the impact of the electron beam. The interlayer bonding force of the titanium alloy is improved, and the composition segregation of the titanium alloy is avoided, especially the segregation of the Fe element produces β spot defects, which affects the strength of the titanium alloy.
上述的一种降低增材制造高强钛合金力学性能各向异性的方法,其特征在于,步骤一中所述球形Ti185合金粉末由以下质量含量的成分组成:Al 1.38%,V 8.00%,Fe4.22%,O 0.19%,余量为钛和不可避免的杂质,且球形Ti185合金粉末的粒度为40μm~150μm。该粒径的球形Ti185合金粉末流动性较好,有利于混合粉末在成形底板上的铺展,提高了铺粉层的均匀性,进而提高了产物钛合金中各组分的均匀性,避免发生成分偏析现象;同时,该粒径的球形Ti185合金粉末有利于提高其在粉末床电子束增材制造成形过程中的熔化速度。The above-mentioned method for reducing the anisotropy of the mechanical properties of high-strength titanium alloys by additive manufacturing is characterized in that the spherical Ti185 alloy powder in step 1 is composed of the following components by mass content: Al 1.38%, V 8.00%, Fe4. 22%, O 0.19%, the balance is titanium and unavoidable impurities, and the particle size of the spherical Ti185 alloy powder is 40 μm to 150 μm. The spherical Ti185 alloy powder with this particle size has good fluidity, which is conducive to the spreading of the mixed powder on the forming base plate, improves the uniformity of the powder layer, and then improves the uniformity of each component in the product titanium alloy, avoiding the occurrence of component Segregation phenomenon; at the same time, the spherical Ti185 alloy powder with this particle size is conducive to improving its melting speed in the forming process of powder bed electron beam additive manufacturing.
上述的一种降低增材制造高强钛合金力学性能各向异性的方法,其特征在于,步骤一中所述铁粉末的粒度为1μm,添加量为球形Ti185合金粉末质量的1.89%。通过控制铁粉末的粒度,有利于铁粉末均匀附着在Ti185合金粉末表面,并且不发生团聚。通常,Ti185合金的铁质量含量为4%~6%,根据化学元素配比计算方法,向本发明的Ti185合金粉末添加1.89%铁粉制备混合粉末,混合粉末中的铁含量还在常规Ti185合金粉末的组分含量范围内,避免引入其他杂质元素,有利于保证钛合金的力学性能。The aforementioned method for reducing the anisotropy of the mechanical properties of high-strength titanium alloys by additive manufacturing is characterized in that the particle size of the iron powder in step 1 is 1 μm, and the addition amount is 1.89% of the mass of the spherical Ti185 alloy powder. By controlling the particle size of the iron powder, it is beneficial for the iron powder to evenly adhere to the surface of the Ti185 alloy powder without agglomeration. Usually, the iron mass content of the Ti185 alloy is 4% to 6%. According to the calculation method of the chemical element ratio, 1.89% iron powder is added to the Ti185 alloy powder of the present invention to prepare a mixed powder. The iron content in the mixed powder is still the same as that of the conventional Ti185 alloy Within the range of the composition content of the powder, the introduction of other impurity elements is avoided, which is conducive to ensuring the mechanical properties of the titanium alloy.
本发明球磨的过程为:向等离子旋转电极气雾化制备的球形Ti185合金粉末中加入铁粉末,然后放入行星式球磨机的球磨罐中,并在球磨罐中加入球磨珠和乙醇,在20r/min的转速下进行球磨4h,得到混合粉末。该过程中加入乙醇以促使铁粉末均匀附着在球形Ti185合金粉末表面。The ball milling process of the present invention is as follows: add iron powder to the spherical Ti185 alloy powder prepared by plasma rotating electrode gas atomization, then put it into the ball milling jar of the planetary ball mill, and add ball milling beads and ethanol in the ball milling jar, at 20r/ The ball milling was carried out for 4 hours at a rotational speed of 1 min to obtain a mixed powder. During this process, ethanol was added to promote the uniform attachment of the iron powder on the surface of the spherical Ti185 alloy powder.
上述的一种降低增材制造高强钛合金力学性能各向异性的方法,其特征在于,步骤二中所述等厚的片层厚度为0.1mm。通过控制片层厚度为0.1mm,以适应电子束对混合粉末的熔化能力。The above-mentioned method for reducing the anisotropy of mechanical properties of high-strength titanium alloys manufactured by additive manufacturing is characterized in that the thickness of the equal-thickness sheet described in step 2 is 0.1 mm. By controlling the thickness of the sheet to 0.1mm, it is suitable for the melting ability of the electron beam to the mixed powder.
上述的一种降低增材制造高强钛合金力学性能各向异性的方法,其特征在于,步骤五中所述熔化扫描的工艺参数为:扫描线间距0.1mm,扫描电流15mA,扫描速度3300mm/s。采用上述熔化扫描成形参数对钛合金球形粉末进行粉末床电子束增材制造钛合金,有效控制了成形过程中各片层的尺寸精度和熔化质量,使得制备的钛合金成形件内部均匀,形状完整,有利于提高钛合金的强度。The above-mentioned method for reducing the anisotropy of the mechanical properties of high-strength titanium alloys by additive manufacturing is characterized in that the process parameters of the melting scan described in step five are: scan line spacing 0.1mm, scan current 15mA, scan speed 3300mm/s . Using the above melting and scanning forming parameters to carry out powder bed electron beam additive manufacturing of titanium alloy spherical powder to titanium alloy, effectively control the dimensional accuracy and melting quality of each layer in the forming process, so that the prepared titanium alloy formed parts are uniform inside and complete in shape , which is beneficial to improve the strength of titanium alloy.
本发明与现有技术相比具有以下优点:Compared with the prior art, the present invention has the following advantages:
1、本发明通过向Ti185合金粉末添加铁粉末进行粉末床电子束增材制造制备钛合金,提高了合金的生长限制因子和凝固温度区间值,有利于钛合金中等轴晶的形成,同时降低β/α转变温度,促进钛合金纳米α强化相析出,从而提高了钛合金的强度,并降低了钛合金力学性能各向异性。1. The present invention prepares titanium alloy by adding iron powder to Ti185 alloy powder for powder bed electron beam additive manufacturing, which improves the growth limiting factor and solidification temperature interval value of the alloy, is conducive to the formation of equiaxed crystals in titanium alloy, and reduces β at the same time /α transition temperature, promotes the precipitation of nano-α strengthening phase of titanium alloy, thereby improving the strength of titanium alloy and reducing the anisotropy of mechanical properties of titanium alloy.
2、本发明通过向Ti185合金粉末添加铁粉末,并根据化学元素配比计算方法控制添加量,不仅促进了钛合金中等轴晶的形成,且添加后混合粉末中的铁含量还在常规Ti185合金粉末的组分含量范围内,避免引入其他杂质元素,有利于保证钛合金的力学性能。2. The present invention not only promotes the formation of equiaxed crystals in the titanium alloy by adding iron powder to the Ti185 alloy powder and controlling the addition amount according to the calculation method of the chemical element ratio, but also the iron content in the mixed powder after the addition is still lower than that of the conventional Ti185 alloy Within the range of the composition content of the powder, the introduction of other impurity elements is avoided, which is conducive to ensuring the mechanical properties of the titanium alloy.
3、本发明的粉末床电子束增材制造过程中通过对铺粉层和成形底板进行预热,有利于产物钛合金内部热应力逐步释放,进而钛合金内部组织趋于均一,同时避免粉末之间粘连,提高了钛合金层间结合力并避免成分偏析,进一步保证了钛合金的强度等力学性能。3. In the powder bed electron beam additive manufacturing process of the present invention, by preheating the powder layer and the forming bottom plate, it is beneficial to gradually release the internal thermal stress of the product titanium alloy, and then the internal structure of the titanium alloy tends to be uniform, while avoiding Inter-adhesion improves the bonding force between titanium alloy layers and avoids component segregation, further ensuring the strength and other mechanical properties of titanium alloys.
4、本发明通过添加铁粉末结合粉末床电子束增材制造,使得制备的钛合金内部为等轴晶,强度高并且显著降低了力学性能各向异性,水平方向的抗拉强度高于1317MPa,竖直方向的抗拉强度高于1303MPa,水平方向的抗拉屈服强度高于1241MPa,竖直方向的抗拉屈服强度高于1222MPa,断后伸长率高于5%,强度各向异性值不高于1.5,可制作为高强度部件,适用范围广泛。4. The present invention combines iron powder with powder bed electron beam additive manufacturing, so that the interior of the prepared titanium alloy is equiaxed, has high strength and significantly reduces the anisotropy of mechanical properties, and the tensile strength in the horizontal direction is higher than 1317MPa. The tensile strength in the vertical direction is higher than 1303MPa, the tensile yield strength in the horizontal direction is higher than 1241MPa, the tensile yield strength in the vertical direction is higher than 1222MPa, the elongation after fracture is higher than 5%, and the strength anisotropy value is not high More than 1.5, it can be made into high-strength parts and has a wide range of applications.
下面通过附图和实施例对本发明的技术方案作进一步的详细描述。The technical solutions of the present invention will be described in further detail below with reference to the drawings and embodiments.
附图说明Description of drawings
图1为本发明实施例1制备的钛合金的光学显微镜图。FIG. 1 is an optical micrograph of the titanium alloy prepared in Example 1 of the present invention.
图2为本发明对比例1制备的钛合金的光学显微镜图。FIG. 2 is an optical microscope image of the titanium alloy prepared in Comparative Example 1 of the present invention.
具体实施方式Detailed ways
本发明实施例1~2和对比例1~2采用的粉末床电子束增材制造设备为赛隆Y150型。The powder bed electron beam additive manufacturing equipment used in Examples 1-2 of the present invention and Comparative Examples 1-2 is Sialon Y150 type.
实施例1Example 1
本实施例包括以下步骤:This embodiment includes the following steps:
步骤一、向球磨罐中放入1kg粒度为40μm~150μm的等离子旋转电极气雾化制备的球形Ti185合金粉末,然后加入18.9g粒度为1μm的铁粉末,再加入球磨珠和乙醇,采用行星式球磨机在20r/min的转速下进行球磨4h,得到混合粉末;所述球形Ti185合金粉末由以下质量含量的成分组成:Al1.38%,V 8.00%,Fe 4.22%,O 0.19%,余量为钛和不可避免的杂质;Step 1. Put 1 kg of spherical Ti185 alloy powder prepared by gas atomization with a plasma rotating electrode with a particle size of 40 μm to 150 μm into the ball mill tank, then add 18.9 g of iron powder with a particle size of 1 μm, then add ball milling beads and ethanol, and use a planetary method The ball mill was milled for 4 hours at a rotating speed of 20r/min to obtain a mixed powder; the spherical Ti185 alloy powder was composed of the following components by mass: Al 1.38%, V 8.00%, Fe 4.22%, O 0.19%, and the balance was Titanium and unavoidable impurities;
步骤二、采用Magics软件绘制目标产物钛合金的三维模型,模型尺寸为80mm×13mm×22mm(长×宽×高),然后进行分层处理,沿着三维模型的高度方向切分成厚度为0.1mm的等厚的片层,并获得切层数据,再对各片层的内部扫描方式和扫描路径进行设计,获得切层扫描数据;所述切层扫描数据包括:扫描线间距为0.1mm,扫描电流为15mA,扫描速度为3300mm/s;Step 2. Use Magics software to draw a three-dimensional model of the target product titanium alloy. The size of the model is 80mm×13mm×22mm (length×width×height), and then carry out layering processing, and cut it into pieces with a thickness of 0.1mm along the height direction of the three-dimensional model slices of equal thickness, and obtain slice data, and then design the internal scanning mode and scan path of each slice to obtain slice scan data; the slice scan data includes: the scan line spacing is 0.1mm, the scan The current is 15mA, and the scanning speed is 3300mm/s;
步骤三、将步骤二获得的切层数据和切层扫描数据导入粉末床电子束增材制造成形设备中,将8kg步骤一中得到的混合粉末装入粉末床电子束增材制造设备的粉箱中,然后调平成形底板并对成形底板进行预热,成形底板的预热温度为720℃,成形底板的尺寸为100mm×100mm×10mm(长×宽×厚);Step 3. Import the slice data and slice scan data obtained in step 2 into the powder bed electron beam additive manufacturing forming equipment, and put 8kg of the mixed powder obtained in step 1 into the powder box of the powder bed electron beam additive manufacturing equipment , then level the forming base plate and preheat the forming base plate, the preheating temperature of the forming base plate is 720°C, and the size of the forming base plate is 100mm×100mm×10mm (length×width×thick);
步骤四、将步骤三中装入粉箱中的混合粉末铺设在预热后的成形底板上形成厚度为0.1mm的铺粉层,然后对铺粉层进行预热,铺粉层的预热温度为720℃;Step 4. Lay the mixed powder loaded into the powder box in step 3 on the preheated forming base plate to form a powder layer with a thickness of 0.1mm, and then preheat the powder layer. The preheating temperature of the powder layer is 720°C;
步骤五、根据步骤三中导入粉末床电子束增材制造成形设备中的切层数据和切层扫描数据,采用电子束对步骤四中经预热后的铺粉层进行熔化扫描,形成单层实体片层,然后将成形底板下降0.1mm;所述熔化扫描的工艺参数为:扫描线间距0.1mm,扫描电流15mA,扫描速度3300mm/s;Step 5. According to the slice data and slice scan data imported into the powder bed electron beam additive manufacturing forming equipment in step 3, the electron beam is used to melt and scan the preheated powder layer in step 4 to form a single layer Solid sheet, and then lower the forming base plate by 0.1mm; the process parameters of the melting scan are: scan line spacing 0.1mm, scan current 15mA, scan speed 3300mm/s;
步骤六、重复步骤四中的铺粉工艺、预热工艺和步骤五中的熔化扫描工艺、成形底板下降工艺,直至各单层实体片层逐层堆积,形成粉末床电子束增材制造成形件,然后待成形底板的温度小于100℃时取出,利用高压气体去除粉末床电子束增材制造成形件表面的残留粉末,得到高强钛合金。Step 6. Repeat the powder spreading process and preheating process in step 4 and the melting scanning process and forming base plate lowering process in step 5 until each single-layer solid sheet is piled up layer by layer to form a powder bed electron beam additive manufacturing shaped part , and then take it out when the temperature of the formed bottom plate is less than 100°C, and use high-pressure gas to remove the residual powder on the surface of the formed part manufactured by powder bed electron beam additive manufacturing to obtain a high-strength titanium alloy.
经检测,本实施例制备的高强钛合金水平方向的抗拉强度为1336MPa,抗拉屈服强度为1270MPa,断后伸长率为9%,竖直方向的抗拉强度为1366MPa,抗拉屈服强度为1256MPa,断后伸长率为6%,抗拉强度各向异值为1.4,抗拉屈服强度各向异值为1.1。其中,各向异值(IPA)根据公式(1)计算。After testing, the horizontal tensile strength of the high-strength titanium alloy prepared in this embodiment is 1336MPa, the tensile yield strength is 1270MPa, the elongation after fracture is 9%, the vertical tensile strength is 1366MPa, and the tensile yield strength is 1256MPa, the elongation after fracture is 6%, the anisotropy of tensile strength is 1.4, and the anisotropy of tensile yield strength is 1.1. Among them, the anisotropic value (IPA) is calculated according to formula (1).
公式(1)中,TH表示水平方向试样的抗拉或屈服强度,单位为MPa;TV表示竖直方向试样的抗拉或屈服强度,单位为MPa。In formula (1), T H represents the tensile or yield strength of the sample in the horizontal direction, in MPa; T V represents the tensile or yield strength of the sample in the vertical direction, in MPa.
图1为本实施例制备的钛合金的光学显微镜图,从图1可以看出,该钛合金沿成形方向为等轴晶,内部为细小α相。Figure 1 is an optical microscope image of the titanium alloy prepared in this example. It can be seen from Figure 1 that the titanium alloy is equiaxed along the forming direction and has a fine α phase inside.
对比例1Comparative example 1
本对比例与实施例1的不同之处在于:本对比例没有步骤一,即未向Ti185合金粉末加入铁粉末,得到Ti185合金。The difference between this comparative example and Example 1 is that this comparative example does not have Step 1, that is, no iron powder is added to Ti185 alloy powder to obtain Ti185 alloy.
经检测,本对比例制备的Ti185合金水平方向的抗拉强度为1075MPa,抗拉屈服强度为1005MPa,断后伸长率为17%,竖直方向的抗拉强度为1131MPa,抗拉屈服强度为1059MPa,断后伸长率为6%,抗拉强度各向异值为5.1,抗拉屈服强度各向异值为5.2。After testing, the horizontal tensile strength of the Ti185 alloy prepared in this comparative example is 1075MPa, the tensile yield strength is 1005MPa, the elongation after fracture is 17%, the vertical tensile strength is 1131MPa, and the tensile yield strength is 1059MPa , The elongation after breaking is 6%, the anisotropy value of the tensile strength is 5.1, and the anisotropy value of the tensile yield strength is 5.2.
图2为本对比例制备的钛合金的光学显微镜图,从图2可以看出,该钛合金沿成形方向为柱状晶组织。FIG. 2 is an optical microscope image of the titanium alloy prepared in this comparative example. It can be seen from FIG. 2 that the titanium alloy has a columnar grain structure along the forming direction.
将实施例1与对比例1进行比较可知,对比例1中未掺入铁粉末的Ti185合金粉末的生长限制因子和凝固温度区间较低,经计算,Ti185合金(铁质量含量为4.22%)的生长限制因子为46.8,凝固温度区间值为96℃;而实施例1中向Ti185合金粉末加入1.89%的铁粉末形成混合钛合金粉末,该钛合金(铁质量含量为6%)的生长限制因子为66.6,凝固温度区间值为129℃。根据凝固的互相依存理论,生长限制因子和凝固温度区间值越高,越容易形成等轴晶。因此,实施例1得到的钛合金内部为等轴晶,而对比例1得到的钛合金内部为柱状晶,且等轴晶的晶粒尺寸、晶内强化相尺寸均小于相应的柱状晶,导致前者强度要高于后者。Comparing Example 1 with Comparative Example 1, it can be seen that the growth limiting factor and solidification temperature range of the Ti185 alloy powder not mixed with iron powder in Comparative Example 1 are relatively low. After calculation, the Ti185 alloy (iron mass content is 4.22%) The growth limiting factor is 46.8, and the solidification temperature interval value is 96 ° C; while adding 1.89% iron powder to the Ti185 alloy powder in Example 1 to form a mixed titanium alloy powder, the growth limiting factor of the titanium alloy (iron mass content is 6%) is 66.6, and the solidification temperature range is 129°C. According to the interdependence theory of solidification, the higher the value of the growth limiting factor and the solidification temperature range, the easier it is to form equiaxed crystals. Therefore, the interior of the titanium alloy obtained in Example 1 is equiaxed crystals, while the interior of the titanium alloy obtained in Comparative Example 1 is columnar crystals, and the grain size of the equiaxed crystals and the size of the intragranular strengthening phase are smaller than the corresponding columnar crystals, resulting in The former is stronger than the latter.
对比例2Comparative example 2
本对比例与实施例1的不同之处在于:本对比例步骤一中加入铁粉末的量为41.1g,钛合金中铁质量含量为8%。The difference between this comparative example and Example 1 is that the amount of iron powder added in step 1 of this comparative example is 41.1 g, and the mass content of iron in the titanium alloy is 8%.
本对比例采用粉末床电子束增材制造的成形过程中,粉末流动性差并且成形过程产生大量飞溅,导致成形工艺终止。In the forming process of powder bed electron beam additive manufacturing in this comparative example, the powder fluidity is poor and a large amount of splash is generated during the forming process, which leads to the termination of the forming process.
将实施例1与对比例2进行比较可知,对比例2中铁粉末的添加量为4.11%,钛合金中铁质量含量高达8%,由于铁粉末含量过高,混合粉末的球形度变差,从而流动性降低。同时,由于铁的熔点和Ti185合金的熔点相差超过100℃,当铁粉末的质量含量增多,导致采用粉末床电子束增材制造技术成形时产生大量飞溅,严重影响成形件的性能,导致成形工艺失败。Comparing Example 1 with Comparative Example 2, it can be seen that the amount of iron powder added in Comparative Example 2 is 4.11%, and the iron mass content in the titanium alloy is as high as 8%. Because the iron powder content is too high, the sphericity of the mixed powder becomes poor, thus flowing reduced sex. At the same time, due to the difference between the melting point of iron and the melting point of Ti185 alloy by more than 100 °C, when the mass content of iron powder increases, a large amount of spatter will be generated when powder bed electron beam additive manufacturing technology is used to form, which seriously affects the performance of the formed part and leads to the formation process fail.
综上,本发明通过向Ti185合金粉末加入铁粉末并控制铁粉末的加入量为6%,提高了合金的生长限制因子和凝固温度区间值,同时混合粉末具有良好的流动性,保证成形过程的进行,并促进钛合金中等轴晶的形成,进而提高了钛合金的强度。In summary, the present invention increases the growth limiting factor and the solidification temperature interval value of the alloy by adding iron powder to the Ti185 alloy powder and controlling the amount of iron powder added to 6%. At the same time, the mixed powder has good fluidity, ensuring the smoothness of the forming process. and promote the formation of equiaxed grains in titanium alloys, thereby improving the strength of titanium alloys.
实施例2Example 2
本实施例包括以下步骤:This embodiment includes the following steps:
步骤一、向球磨罐中放入1kg粒度为40μm~150μm的等离子旋转电极气雾化制备的球形Ti185合金粉末,然后加入18.9g粒度为1μm的铁粉末,再加入球磨珠和乙醇,采用行星式球磨机在20r/min的转速下进行球磨4h,得到混合粉末;所述球形Ti185合金粉末由以下质量含量的成分组成:Al1.38%,V 8.00%,Fe 4.22%,O 0.19%,余量为钛和不可避免的杂质;Step 1. Put 1 kg of spherical Ti185 alloy powder prepared by gas atomization with a plasma rotating electrode with a particle size of 40 μm to 150 μm into the ball mill tank, then add 18.9 g of iron powder with a particle size of 1 μm, then add ball milling beads and ethanol, and use a planetary method The ball mill was milled for 4 hours at a rotating speed of 20r/min to obtain a mixed powder; the spherical Ti185 alloy powder was composed of the following components by mass: Al 1.38%, V 8.00%, Fe 4.22%, O 0.19%, and the balance was Titanium and unavoidable impurities;
步骤二、采用Magics软件绘制目标产物钛合金的三维模型,模型尺寸为80mm×13mm×22mm(长×宽×高),然后进行分层处理,沿着三维模型的高度方向切分成厚度为0.1mm的等厚的片层,并获得切层数据,再对各片层的内部扫描方式和扫描路径进行设计,获得切层扫描数据;所述切层扫描数据包括:扫描线间距为0.1mm,扫描电流为15mA,扫描速度为3300mm/s;Step 2. Use Magics software to draw a three-dimensional model of the target product titanium alloy. The size of the model is 80mm×13mm×22mm (length×width×height), and then carry out layering processing, and cut it into pieces with a thickness of 0.1mm along the height direction of the three-dimensional model slices of equal thickness, and obtain slice data, and then design the internal scanning mode and scan path of each slice to obtain slice scan data; the slice scan data includes: the scan line spacing is 0.1mm, the scan The current is 15mA, and the scanning speed is 3300mm/s;
步骤三、将步骤二获得的切层数据和切层扫描数据导入粉末床电子束增材制造成形设备中,将8kg步骤一中得到的混合粉末装入粉末床电子束增材制造设备的粉箱中,然后调平成形底板并对成形底板进行预热,成形底板的预热温度为700℃,成形底板的尺寸为100mm×100mm×10mm(长×宽×厚);Step 3. Import the slice data and slice scan data obtained in step 2 into the powder bed electron beam additive manufacturing forming equipment, and put 8kg of the mixed powder obtained in step 1 into the powder box of the powder bed electron beam additive manufacturing equipment , then level the forming base plate and preheat the forming base plate, the preheating temperature of the forming base plate is 700°C, and the size of the forming base plate is 100mm×100mm×10mm (length×width×thick);
步骤四、将步骤三中装入粉箱中的混合粉末铺设在预热后的成形底板上形成厚度为0.1mm的铺粉层,然后对铺粉层进行预热,铺粉层的预热温度为700℃;Step 4. Lay the mixed powder loaded into the powder box in step 3 on the preheated forming base plate to form a powder layer with a thickness of 0.1mm, and then preheat the powder layer. The preheating temperature of the powder layer is 700°C;
步骤五、根据步骤三中导入粉末床电子束增材制造成形设备中的切层数据和切层扫描数据,采用电子束对步骤四中经预热后的铺粉层进行熔化扫描,形成单层实体片层,然后将成形底板下降0.1mm;所述熔化扫描的工艺参数为:扫描线间距0.1mm,扫描电流15mA,扫描速度3300mm/s;Step 5. According to the slice data and slice scan data imported into the powder bed electron beam additive manufacturing forming equipment in step 3, the electron beam is used to melt and scan the preheated powder layer in step 4 to form a single layer Solid sheet, and then lower the forming base plate by 0.1mm; the process parameters of the melting scan are: scan line spacing 0.1mm, scan current 15mA, scan speed 3300mm/s;
步骤六、重复步骤四中的铺粉工艺、预热工艺和步骤五中的熔化扫描工艺、成形底板下降工艺,直至各单层实体片层逐层堆积,形成粉末床电子束增材制造成形件,然后待成形底板的温度小于100℃时取出,利用高压气体去除粉末床电子束增材制造成形件表面的残留粉末,得到高强钛合金。Step 6. Repeat the powder spreading process and preheating process in step 4 and the melting scanning process and forming base plate lowering process in step 5 until each single-layer solid sheet is piled up layer by layer to form a powder bed electron beam additive manufacturing shaped part , and then take it out when the temperature of the formed bottom plate is less than 100°C, and use high-pressure gas to remove the residual powder on the surface of the formed part manufactured by powder bed electron beam additive manufacturing to obtain a high-strength titanium alloy.
经检测,本实施例制备的高强钛合金水平方向的抗拉强度为1317MPa,抗拉屈服强度为1241MPa,断后伸长率为7%,竖直方向的抗拉强度为1303MPa,抗拉屈服强度为1222MPa,断后伸长率为5%,抗拉强度各向异值为1.1,抗拉屈服强度各向异值为1.5。After testing, the tensile strength of the high-strength titanium alloy prepared in this embodiment in the horizontal direction is 1317MPa, the tensile yield strength is 1241MPa, the elongation after fracture is 7%, the tensile strength in the vertical direction is 1303MPa, and the tensile yield strength is 1222MPa, the elongation after fracture is 5%, the anisotropy of tensile strength is 1.1, and the anisotropy of tensile yield strength is 1.5.
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化,均仍属于本发明技术方案的保护范围内。The above descriptions are only preferred embodiments of the present invention, and do not limit the present invention in any way. All simple modifications, changes and equivalent changes made to the above embodiments according to the technical essence of the invention still belong to the protection scope of the technical solution of the invention.
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